Abstract：The abyssal sediments contain a variety of mineral resources. The accurate determination of major and minor components in abyssal sediments is of great significance for the development and utilization of mineral resources in abyssal sediments. Twenty major and minor components in abyssal sediments (including Na2O, MgO, Al2O3, SiO2, P2O5, SO3, Cl, K2O, CaO, TiO2, MnO, Fe2O3, Ba, Cu, Ni, Sr, V, Y, Zn and Zr) were accurately determined by X-ray fluorescence spectrometry (XRF) with fusion sample preparation. The contents of SO3 and Cl (0.10%-3.00%) in abyssal sediment samples were high, while the contents of micro elements (Cu, Ni, Sr, V, Y, Zn and Zr) were usually in range of 5-600μg/g. In order to accurately determine these components, the fusion sample preparation conditions were discussed in detail. Since SO3 and Cl were easily volatilized during sample fusion, the samples were pre-oxidized for twice at 600℃ and 700℃, respectively, which effectively prevented the volatilization loss of SO3 and Cl in sample fusion. The fusion temperature in experiments was selected as 1100℃. The mass of sample and mixed flux (m(Li2B4O7)∶m(LiBO2)=67∶33) was 0.7000g and 7.000g, respectively. The quality of melt was good. In order to make the calibration curves of elements have a certain content range and meanwhile appropriate content gradient, the calibration sample was prepared using certified reference materials of abyssal sediment (GBW07313-GBW07316) and ocean sediments (GBW07333-GBW07336) with mass ratio of 1∶1. Moreover, the certified reference material of abyssal sediment (GBW07316) was also mixed with high-purity sodium sulfate and sodium chloride in certain proportion to prepare synthetic calibration samples. The mass fraction of SO3 and Cl was 1.00% and 5.00%, respectively. The overlapping effect of spectral lines was corrected by empirical coefficient method, and the matrix effect was corrected by theoretical α coefficient. Under the selected experimental conditions, 12 melts were prepared using GBW07316 standard sample for the precision test. The relative standard deviations (RSD) of determination results were measured between 0.10% and 4.6%. The proposed method was applied for the determination of standard sample and actual sample. The determination results of major and minor components were consistent with the certified values for standard sample and those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES) for actual sample.
王川. 熔融制样-X射线荧光光谱法测定深海沉积物中20种主次组分[J]. 冶金分析, 2020, 40(6): 49-55.
WANG Chuan. Determination of twenty major and minor components in abyssal sediments by X-ray fluorescence spectrometry with fusion sample preparation. , 2020, 40(6): 49-55.
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